# ic991312+.cif data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84112074' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript (IC 991312+) submitted to Inorg. Chem. Xiao-Ming Chen ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; A new type of molecular ladders organised into novel 3-D molecular networks via multiple polythreading of the lateral arms into the squares of adjacent ladders (Paper No. IC991312+) ; loop_ _publ_author_name _publ_author_address 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Hong-Ji' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; #============================================================ data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H46 Cu2 N8 O18' _chemical_formula_weight 1101.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.023(3) _cell_length_b 15.398(8) _cell_length_c 14.315(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.02 _cell_angle_gamma 90.00 _cell_volume 2335.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour 'deep blue' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.952 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% none _diffrn_reflns_number 5341 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.02 _reflns_number_total 5085 _reflns_number_gt 3782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97, V.5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+1.7031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5085 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 1.001 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.14247(3) 0.16817(2) 0.14087(3) 0.02449(12) Uani 1 d . . . N1 N 0.3254(2) 0.16933(16) 0.14284(18) 0.0260(5) Uani 1 d . . . N2 N 0.9633(2) 0.16155(16) 0.14646(18) 0.0281(5) Uani 1 d . . . N3 N 0.1050(2) 0.29113(16) 0.08745(19) 0.0296(6) Uani 1 d . . . O1 O 0.17880(19) 0.06489(13) 0.22800(15) 0.0292(5) Uani 1 d . . . O2 O 0.2128(2) 0.18088(14) 0.31948(17) 0.0402(6) Uani 1 d . . . O3 O 0.4146(4) -0.1025(2) 0.6397(2) 0.0997(15) Uani 1 d . . . H3 H 0.4288 -0.1418 0.6295 0.050 Uiso 1 d R . . C1 C 0.3977(3) 0.2400(2) 0.1574(2) 0.0330(7) Uani 1 d . . . H1A H 0.3604 0.2942 0.1675 0.080 Uiso 1 d R . . C2 C 0.5220(3) 0.2390(2) 0.1591(3) 0.0335(7) Uani 1 d . . . H2A H 0.5702 0.2918 0.1691 0.080 Uiso 1 d R . . C3 C 0.5782(3) 0.1616(2) 0.1468(2) 0.0276(6) Uani 1 d . . . C4 C 0.5039(3) 0.0878(2) 0.1327(2) 0.0316(7) Uani 1 d . . . H4A H 0.5394 0.0325 0.1239 0.080 Uiso 1 d R . . C5 C 0.37959(19) 0.09410(14) 0.13131(17) 0.0307(7) Uani 1 d . . . H5A H 0.3294 0.0422 0.1219 0.080 Uiso 1 d R . . C6 C 0.88395(19) 0.10077(14) 0.09839(17) 0.0337(7) Uani 1 d R . . H6A H 0.9151 0.0578 0.0622 0.080 Uiso 1 d R . . C7 C 0.7596(3) 0.0969(2) 0.0986(3) 0.0351(7) Uani 1 d . . . H7A H 0.7059 0.0519 0.0633 0.080 Uiso 1 d R . . C8 C 0.7122(3) 0.15838(19) 0.1496(2) 0.0269(6) Uani 1 d . . . C9 C 0.7963(3) 0.2190(2) 0.2017(2) 0.0333(7) Uani 1 d . . . H9A H 0.7687 0.2615 0.2404 0.080 Uiso 1 d R . . C10 C 0.9184(3) 0.2187(2) 0.1984(2) 0.0348(7) Uani 1 d . . . H10A H 0.9748 0.2616 0.2353 0.080 Uiso 1 d R . . C11 C 0.0422(4) 0.3042(2) -0.0044(3) 0.0433(8) Uani 1 d . . . H11A H 0.0248 0.2551 -0.0474 0.080 Uiso 1 d R . . C12 C 0.0006(4) 0.3842(2) -0.0408(3) 0.0461(9) Uani 1 d . . . H12A H -0.0443 0.3905 -0.1082 0.080 Uiso 1 d R . . C13 C 0.0224(3) 0.45618(19) 0.0185(2) 0.0299(7) Uani 1 d . . . C14 C 0.0893(3) 0.4424(2) 0.1138(2) 0.0385(8) Uani 1 d . . . H14A H 0.1087 0.4904 0.1582 0.080 Uiso 1 d R . . C15 C 0.1277(3) 0.3603(2) 0.1449(2) 0.0368(7) Uani 1 d . . . H15A H 0.1737 0.3522 0.2118 0.080 Uiso 1 d R . . C16 C 0.2175(3) 0.1009(2) 0.3115(2) 0.0296(7) Uani 1 d . . . C17 C 0.2693(3) 0.0453(2) 0.3965(2) 0.0310(7) Uani 1 d . . . C18 C 0.3367(3) 0.0819(2) 0.4836(2) 0.0407(8) Uani 1 d . . . H18A H 0.3505 0.1435 0.4877 0.080 Uiso 1 d R . . C19 C 0.3849(4) 0.0312(2) 0.5641(3) 0.0499(10) Uani 1 d . . . H19A H 0.4319 0.0571 0.6242 0.080 Uiso 1 d R . . C20 C 0.3664(4) -0.0568(3) 0.5587(3) 0.0551(11) Uani 1 d . . . C21 C 0.2992(4) -0.0944(2) 0.4728(3) 0.0467(9) Uani 1 d . . . H21A H 0.2855 -0.1560 0.4694 0.080 Uiso 1 d R . . C22 C 0.2514(3) -0.0434(2) 0.3924(2) 0.0379(8) Uani 1 d . . . H22A H 0.2051 -0.0699 0.3324 0.080 Uiso 1 d R . . O1W O 0.1097(2) 0.10048(14) -0.00499(16) 0.0368(5) Uani 1 d . . . H1WA H 0.1647 0.1138 -0.0304 0.050 Uiso 1 d R . . H1WB H 0.0428 0.0957 -0.0368 0.050 Uiso 1 d R . . O3W O 0.2756(3) 0.34314(18) 0.3942(2) 0.0596(8) Uani 1 d . . . H3WA H 0.2627 0.2916 0.3911 0.050 Uiso 1 d R . . H3WB H 0.3390 0.3469 0.4043 0.050 Uiso 1 d R . . O2W O 0.1111(2) -0.09808(17) 0.14511(18) 0.0514(7) Uani 1 d . . . H2WA H 0.1682 -0.1185 0.1370 0.050 Uiso 1 d R . . H2WB H 0.1348 -0.0543 0.1680 0.050 Uiso 1 d R . . N4 N 0.3978(4) -0.1793(2) 0.1109(3) 0.0604(9) Uani 1 d . . . O4 O 0.2968(3) -0.2120(2) 0.1115(3) 0.0761(9) Uani 1 d . . . O5 O 0.4727(3) -0.2253(3) 0.0862(3) 0.0941(12) Uani 1 d . . . O6 O 0.4203(5) -0.1065(2) 0.1332(5) 0.155(2) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01603(17) 0.02444(19) 0.0330(2) 0.00597(16) 0.00672(13) 0.00309(14) N1 0.0173(11) 0.0284(12) 0.0329(13) 0.0050(11) 0.0079(9) 0.0012(10) N2 0.0187(11) 0.0289(13) 0.0359(14) 0.0029(11) 0.0065(10) 0.0038(10) N3 0.0240(12) 0.0272(13) 0.0378(15) 0.0070(11) 0.0090(11) 0.0045(10) O1 0.0274(10) 0.0297(11) 0.0283(11) 0.0043(9) 0.0041(9) 0.0009(8) O2 0.0474(14) 0.0286(13) 0.0409(13) 0.0025(10) 0.0062(11) 0.0045(10) O3 0.190(4) 0.0499(19) 0.0336(16) 0.0123(14) -0.011(2) 0.017(2) C1 0.0269(15) 0.0268(16) 0.0451(19) 0.0015(14) 0.0095(14) 0.0035(12) C2 0.0244(14) 0.0261(15) 0.050(2) 0.0010(14) 0.0112(14) -0.0035(12) C3 0.0204(13) 0.0339(16) 0.0292(15) 0.0015(13) 0.0080(11) 0.0019(12) C4 0.0232(14) 0.0302(16) 0.0440(18) -0.0007(14) 0.0135(13) 0.0013(12) C5 0.0241(14) 0.0285(16) 0.0400(18) 0.0001(13) 0.0099(13) 0.0008(12) C6 0.0250(15) 0.0313(16) 0.048(2) -0.0039(14) 0.0150(14) 0.0010(13) C7 0.0242(15) 0.0345(17) 0.049(2) -0.0070(15) 0.0146(14) -0.0030(13) C8 0.0199(13) 0.0299(16) 0.0306(15) 0.0036(12) 0.0065(11) -0.0009(11) C9 0.0217(14) 0.0409(18) 0.0381(18) -0.0075(14) 0.0099(13) 0.0010(13) C10 0.0227(14) 0.0416(19) 0.0401(18) -0.0071(15) 0.0089(13) -0.0024(13) C11 0.056(2) 0.0288(17) 0.0397(19) 0.0018(14) 0.0049(17) 0.0079(15) C12 0.063(2) 0.0331(18) 0.0355(19) 0.0058(15) 0.0016(17) 0.0122(16) C13 0.0262(15) 0.0272(16) 0.0363(17) 0.0045(13) 0.0088(13) 0.0058(12) C14 0.0450(19) 0.0277(16) 0.0366(18) 0.0008(14) 0.0006(15) 0.0066(14) C15 0.0377(18) 0.0331(16) 0.0346(17) 0.0059(14) 0.0019(14) 0.0066(14) C16 0.0240(14) 0.0327(17) 0.0336(17) 0.0036(13) 0.0106(12) 0.0020(12) C17 0.0307(16) 0.0309(16) 0.0316(16) 0.0012(13) 0.0088(13) 0.0030(13) C18 0.0461(19) 0.0368(18) 0.0354(18) 0.0000(14) 0.0051(15) 0.0045(15) C19 0.067(3) 0.045(2) 0.0301(18) -0.0028(16) 0.0002(17) 0.0069(18) C20 0.086(3) 0.047(2) 0.0274(18) 0.0076(16) 0.0073(19) 0.015(2) C21 0.070(3) 0.0290(17) 0.0365(19) 0.0051(15) 0.0070(18) 0.0025(17) C22 0.0460(19) 0.0352(18) 0.0289(17) 0.0017(14) 0.0042(14) 0.0017(15) O1W 0.0284(11) 0.0437(13) 0.0368(12) -0.0040(10) 0.0066(9) -0.0003(10) O3W 0.0512(16) 0.0568(18) 0.0694(19) -0.0178(15) 0.0143(14) 0.0012(13) O2W 0.0435(14) 0.0449(15) 0.0567(17) -0.0079(13) -0.0015(12) -0.0013(12) N4 0.073(3) 0.044(2) 0.059(2) 0.0136(17) 0.0099(19) 0.0029(19) O4 0.074(2) 0.081(2) 0.082(2) 0.0063(19) 0.0365(19) -0.0001(19) O5 0.065(2) 0.114(3) 0.110(3) -0.023(3) 0.036(2) -0.007(2) O6 0.166(5) 0.037(2) 0.220(6) -0.006(3) -0.018(4) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.992(2) . ? Cu1 N2 2.001(2) 1_455 ? Cu1 N1 2.009(2) . ? Cu1 N3 2.041(3) . ? Cu1 O1W 2.272(2) . ? Cu1 O2 2.466(3) . ? N1 C1 1.330(4) . ? N1 C5 1.334(3) . ? N2 C10 1.332(4) . ? N2 C6 1.335(3) . ? N2 Cu1 2.001(2) 1_655 ? N3 C11 1.322(4) . ? N3 C15 1.327(4) . ? O1 C16 1.279(4) . ? O1 O2W 2.788(3) . ? O2 C16 1.240(4) . ? O2 O3W 2.731(4) . ? O3 C20 1.335(4) . ? O3 O5 2.881(6) 4_556 ? C1 C2 1.364(4) . ? C2 C3 1.376(4) . ? C3 C4 1.382(4) . ? C3 C8 1.467(4) . ? C4 C5 1.368(3) . ? C6 C7 1.373(4) . ? C7 C8 1.383(4) . ? C8 C9 1.380(4) . ? C9 C10 1.360(4) . ? C11 C12 1.367(5) . ? C12 C13 1.376(5) . ? C13 C14 1.376(4) . ? C13 C13 1.484(6) 3_565 ? C14 C15 1.368(4) . ? C16 C17 1.468(4) . ? C17 C22 1.380(4) . ? C17 C18 1.383(5) . ? C18 C19 1.372(5) . ? C19 C20 1.369(5) . ? C20 C21 1.376(5) . ? C21 C22 1.372(5) . ? O1W O2W 2.694(3) 3 ? O1W O3W 2.763(4) 4_565 ? O3W O5 2.908(5) 2_655 ? O2W O4 2.836(4) . ? N4 O6 1.174(5) . ? N4 O5 1.212(5) . ? N4 O4 1.224(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 87.96(9) . 1_455 ? O1 Cu1 N1 88.32(9) . . ? N2 Cu1 N1 176.17(10) 1_455 . ? O1 Cu1 N3 163.73(10) . . ? N2 Cu1 N3 87.85(10) 1_455 . ? N1 Cu1 N3 95.47(10) . . ? O1 Cu1 O1W 99.36(9) . . ? N2 Cu1 O1W 96.03(9) 1_455 . ? N1 Cu1 O1W 85.49(9) . . ? N3 Cu1 O1W 96.71(10) . . ? O1 Cu1 O2 57.52(8) . . ? N2 Cu1 O2 89.65(9) 1_455 . ? N1 Cu1 O2 87.58(9) . . ? N3 Cu1 O2 106.74(9) . . ? O1W Cu1 O2 156.08(8) . . ? C1 N1 C5 117.4(2) . . ? C1 N1 Cu1 124.4(2) . . ? C5 N1 Cu1 118.20(17) . . ? C10 N2 C6 117.3(2) . . ? C10 N2 Cu1 120.8(2) . 1_655 ? C6 N2 Cu1 121.91(18) . 1_655 ? C11 N3 C15 116.8(3) . . ? C11 N3 Cu1 120.7(2) . . ? C15 N3 Cu1 121.9(2) . . ? C16 O1 Cu1 101.34(18) . . ? C16 O1 O2W 140.23(19) . . ? Cu1 O1 O2W 117.91(11) . . ? C16 O2 Cu1 80.47(19) . . ? C16 O2 O3W 158.9(2) . . ? Cu1 O2 O3W 116.87(11) . . ? C20 O3 O5 108.5(3) . 4_556 ? N1 C1 C2 123.3(3) . . ? C1 C2 C3 119.5(3) . . ? C2 C3 C4 117.4(3) . . ? C2 C3 C8 120.7(3) . . ? C4 C3 C8 121.9(3) . . ? C5 C4 C3 119.7(3) . . ? N1 C5 C4 122.7(2) . . ? N2 C6 C7 122.8(2) . . ? C6 C7 C8 119.6(3) . . ? C9 C8 C7 116.9(3) . . ? C9 C8 C3 120.9(3) . . ? C7 C8 C3 122.2(3) . . ? C10 C9 C8 120.2(3) . . ? N2 C10 C9 123.0(3) . . ? N3 C11 C12 123.1(3) . . ? C11 C12 C13 120.5(3) . . ? C12 C13 C14 116.3(3) . . ? C12 C13 C13 121.8(4) . 3_565 ? C14 C13 C13 121.9(4) . 3_565 ? C15 C14 C13 119.8(3) . . ? N3 C15 C14 123.5(3) . . ? O2 C16 O1 120.4(3) . . ? O2 C16 C17 121.3(3) . . ? O1 C16 C17 118.4(3) . . ? C22 C17 C18 118.4(3) . . ? C22 C17 C16 121.6(3) . . ? C18 C17 C16 120.0(3) . . ? C19 C18 C17 120.9(3) . . ? C20 C19 C18 119.8(3) . . ? O3 C20 C19 117.0(4) . . ? O3 C20 C21 122.8(4) . . ? C19 C20 C21 120.1(3) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C17 120.9(3) . . ? Cu1 O1W O2W 124.92(11) . 3 ? Cu1 O1W O3W 112.05(11) . 4_565 ? O2W O1W O3W 102.00(12) 3 4_565 ? O2 O3W O5 80.69(12) . 2_655 ? O1 O2W O4 120.54(12) . . ? O6 N4 O5 121.9(5) . . ? O6 N4 O4 121.0(5) . . ? O5 N4 O4 117.1(4) . . ? N4 O4 O2W 116.6(3) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.515 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.071 #===END data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H46 Co2 N8 O18' _chemical_formula_weight 1092.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1040(10) _cell_length_b 15.4900(10) _cell_length_c 14.3900(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.02(2) _cell_angle_gamma 90.00 _cell_volume 2379.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.862 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% none _diffrn_reflns_number 9374 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 23.33 _reflns_number_total 3401 _reflns_number_gt 2336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97, V.5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3401 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.14247(4) 0.16816(3) 0.14076(4) 0.0244(2) Uani 1 d . . . N1 N 0.3253(3) 0.1692(2) 0.1435(2) 0.0346(8) Uani 1 d . . . N2 N 0.9633(3) 0.1615(2) 0.1456(3) 0.0352(9) Uani 1 d . . . N3 N 0.1051(3) 0.2903(2) 0.0872(3) 0.0382(9) Uani 1 d . . . O1 O 0.1784(2) 0.06491(18) 0.2276(2) 0.0384(7) Uani 1 d . . . O2 O 0.2122(3) 0.18133(19) 0.3194(2) 0.0492(8) Uani 1 d . . . O3 O 0.4141(5) -0.1030(3) 0.6397(3) 0.1155(18) Uani 1 d . . . H3 H 0.4283 -0.1423 0.6294 0.050 Uiso 1 d R . . C1 C 0.3973(4) 0.2402(3) 0.1570(3) 0.0422(12) Uani 1 d . . . H1A H 0.3600 0.2945 0.1672 0.080 Uiso 1 d R . . C2 C 0.5216(4) 0.2385(3) 0.1594(3) 0.0440(12) Uani 1 d . . . H2A H 0.5698 0.2913 0.1694 0.080 Uiso 1 d R . . C3 C 0.5781(4) 0.1613(3) 0.1465(3) 0.0363(10) Uani 1 d . . . C4 C 0.5039(4) 0.0876(3) 0.1328(3) 0.0407(11) Uani 1 d . . . H4A H 0.5395 0.0323 0.1241 0.080 Uiso 1 d R . . C5 C 0.3805(3) 0.0943(2) 0.1315(2) 0.0404(11) Uani 1 d . . . H5A H 0.3303 0.0424 0.1221 0.080 Uiso 1 d R . . C6 C 0.8848(3) 0.1010(2) 0.0986(2) 0.0462(12) Uani 1 d R . . H6A H 0.9160 0.0581 0.0624 0.080 Uiso 1 d R . . C7 C 0.7600(4) 0.0971(3) 0.0999(3) 0.0436(12) Uani 1 d . . . H7A H 0.7063 0.0520 0.0647 0.080 Uiso 1 d R . . C8 C 0.7131(4) 0.1585(3) 0.1493(3) 0.0346(10) Uani 1 d . . . C9 C 0.7966(4) 0.2194(3) 0.2016(3) 0.0426(12) Uani 1 d . . . H9A H 0.7690 0.2619 0.2403 0.080 Uiso 1 d R . . C10 C 0.9188(4) 0.2183(3) 0.1977(3) 0.0435(12) Uani 1 d . . . H10A H 0.9753 0.2612 0.2346 0.080 Uiso 1 d R . . C11 C 0.0425(5) 0.3041(3) -0.0049(4) 0.0520(13) Uani 1 d . . . H11A H 0.0251 0.2550 -0.0479 0.080 Uiso 1 d R . . C12 C -0.0003(5) 0.3842(3) -0.0413(3) 0.0533(13) Uani 1 d . . . H12A H -0.0452 0.3905 -0.1087 0.080 Uiso 1 d R . . C13 C 0.0224(4) 0.4565(3) 0.0184(3) 0.0379(11) Uani 1 d . . . C14 C 0.0878(4) 0.4424(3) 0.1136(3) 0.0468(12) Uani 1 d . . . H14A H 0.1072 0.4904 0.1580 0.080 Uiso 1 d R . . C15 C 0.1275(4) 0.3601(3) 0.1458(3) 0.0467(12) Uani 1 d . . . H15A H 0.1735 0.3519 0.2126 0.080 Uiso 1 d R . . C16 C 0.2176(4) 0.1011(3) 0.3116(3) 0.0382(11) Uani 1 d . . . C17 C 0.2693(4) 0.0452(3) 0.3971(3) 0.0369(11) Uani 1 d . . . C18 C 0.3362(4) 0.0823(3) 0.4834(3) 0.0485(12) Uani 1 d . . . H18A H 0.3501 0.1439 0.4875 0.080 Uiso 1 d R . . C19 C 0.3846(5) 0.0313(3) 0.5639(4) 0.0596(15) Uani 1 d . . . H19A H 0.4316 0.0572 0.6240 0.080 Uiso 1 d R . . C20 C 0.3662(5) -0.0564(3) 0.5581(4) 0.0636(15) Uani 1 d . . . C21 C 0.2990(5) -0.0953(3) 0.4719(3) 0.0576(14) Uani 1 d . . . H21A H 0.2853 -0.1569 0.4685 0.080 Uiso 1 d R . . C22 C 0.2519(4) -0.0439(3) 0.3926(3) 0.0471(12) Uani 1 d . . . H22A H 0.2056 -0.0704 0.3326 0.080 Uiso 1 d R . . O1W O 0.1103(3) 0.10082(19) -0.0053(2) 0.0482(8) Uani 1 d . . . H1WA H 0.1653 0.1141 -0.0307 0.050 Uiso 1 d R . . H1WB H 0.0434 0.0960 -0.0372 0.050 Uiso 1 d R . . O3W O 0.2757(3) 0.3430(2) 0.3941(3) 0.0735(11) Uani 1 d . . . H3WA H 0.2628 0.2915 0.3910 0.050 Uiso 1 d R . . H3WB H 0.3391 0.3468 0.4042 0.050 Uiso 1 d R . . O2W O 0.1105(3) -0.0987(2) 0.1453(2) 0.0651(10) Uani 1 d . . . H2WA H 0.1676 -0.1191 0.1372 0.050 Uiso 1 d R . . H2WB H 0.1342 -0.0549 0.1682 0.050 Uiso 1 d R . . N4 N 0.3982(5) -0.1788(3) 0.1114(4) 0.0717(14) Uani 1 d . . . O4 O 0.2961(4) -0.2116(3) 0.1110(3) 0.0867(13) Uani 1 d . . . O5 O 0.4737(4) -0.2248(3) 0.0869(4) 0.1074(17) Uani 1 d . . . O6 O 0.4217(6) -0.1059(3) 0.1334(5) 0.171(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0144(3) 0.0229(3) 0.0355(4) 0.0064(3) 0.0060(2) 0.0033(2) N1 0.0273(18) 0.032(2) 0.043(2) 0.0023(18) 0.0077(17) 0.0016(17) N2 0.0261(18) 0.034(2) 0.045(2) 0.0016(18) 0.0094(17) 0.0052(16) N3 0.032(2) 0.036(2) 0.045(3) 0.0047(19) 0.0075(19) 0.0037(17) O1 0.0324(16) 0.0371(17) 0.0420(19) -0.0003(15) 0.0039(14) 0.0014(13) O2 0.054(2) 0.034(2) 0.056(2) 0.0026(15) 0.0097(17) 0.0046(15) O3 0.213(5) 0.058(3) 0.049(3) 0.015(2) -0.009(3) 0.020(3) C1 0.030(2) 0.038(3) 0.058(3) 0.000(2) 0.011(2) 0.005(2) C2 0.029(2) 0.037(3) 0.066(3) 0.002(2) 0.013(2) -0.002(2) C3 0.027(2) 0.039(3) 0.042(3) 0.003(2) 0.009(2) 0.002(2) C4 0.026(2) 0.038(3) 0.058(3) -0.004(2) 0.013(2) 0.000(2) C5 0.033(2) 0.033(3) 0.054(3) 0.002(2) 0.010(2) -0.001(2) C6 0.035(3) 0.038(3) 0.067(3) -0.005(3) 0.017(3) 0.002(2) C7 0.032(2) 0.037(3) 0.064(3) -0.009(2) 0.017(2) -0.003(2) C8 0.028(2) 0.033(3) 0.042(3) 0.006(2) 0.009(2) 0.0047(19) C9 0.029(2) 0.045(3) 0.054(3) -0.010(2) 0.011(2) 0.001(2) C10 0.033(2) 0.044(3) 0.053(3) -0.006(2) 0.012(2) -0.003(2) C11 0.068(3) 0.038(3) 0.041(3) 0.002(2) 0.001(3) 0.010(2) C12 0.071(4) 0.038(3) 0.043(3) 0.005(2) 0.002(3) 0.013(2) C13 0.033(2) 0.035(3) 0.046(3) 0.009(2) 0.012(2) 0.0072(19) C14 0.051(3) 0.033(3) 0.050(3) 0.001(2) 0.004(3) 0.008(2) C15 0.041(3) 0.044(3) 0.047(3) 0.007(3) -0.002(2) 0.009(2) C16 0.026(2) 0.037(3) 0.055(3) 0.000(2) 0.017(2) 0.001(2) C17 0.036(3) 0.040(3) 0.035(3) 0.005(2) 0.010(2) 0.005(2) C18 0.053(3) 0.044(3) 0.043(3) -0.001(2) 0.003(3) 0.001(2) C19 0.076(4) 0.047(3) 0.047(3) -0.004(3) 0.003(3) 0.003(3) C20 0.085(4) 0.050(4) 0.051(4) 0.013(3) 0.011(3) 0.014(3) C21 0.079(4) 0.044(3) 0.043(3) 0.002(3) 0.006(3) -0.004(3) C22 0.054(3) 0.044(3) 0.039(3) 0.003(2) 0.008(2) 0.002(2) O1W 0.0344(17) 0.054(2) 0.053(2) -0.0033(16) 0.0071(15) -0.0028(15) O3W 0.059(2) 0.067(3) 0.092(3) -0.022(2) 0.017(2) -0.0015(19) O2W 0.053(2) 0.056(2) 0.073(3) -0.0112(19) -0.0042(19) -0.0009(17) N4 0.082(4) 0.053(4) 0.072(4) 0.012(3) 0.008(3) 0.000(3) O4 0.077(3) 0.092(3) 0.099(3) 0.009(3) 0.039(3) -0.001(3) O5 0.075(3) 0.130(4) 0.126(4) -0.022(3) 0.041(3) 0.000(3) O6 0.193(6) 0.041(3) 0.235(7) -0.007(4) -0.018(5) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.001(3) . ? Co1 N2 2.012(3) 1_455 ? Co1 N1 2.020(3) . ? Co1 N3 2.041(3) . ? Co1 O1W 2.285(3) . ? Co1 O2 2.480(3) . ? N1 C1 1.341(5) . ? N1 C5 1.344(4) . ? N2 C6 1.330(4) . ? N2 C10 1.336(5) . ? N2 Co1 2.012(3) 1_655 ? N3 C11 1.333(6) . ? N3 C15 1.352(6) . ? O1 C16 1.294(5) . ? O1 O2W 2.810(4) . ? O2 C16 1.251(5) . ? O2 O3W 2.740(4) . ? O3 C20 1.355(6) . ? O3 O5 2.900(7) 4_556 ? C1 C2 1.372(6) . ? C2 C3 1.386(6) . ? C3 C4 1.389(6) . ? C3 C8 1.489(5) . ? C4 C5 1.370(5) . ? C6 C7 1.393(5) . ? C7 C8 1.373(6) . ? C8 C9 1.389(6) . ? C9 C10 1.373(5) . ? C11 C12 1.379(6) . ? C12 C13 1.391(6) . ? C13 C14 1.380(6) . ? C13 C13 1.483(8) 3_565 ? C14 C15 1.385(6) . ? C16 C17 1.484(6) . ? C17 C18 1.384(6) . ? C17 C22 1.393(6) . ? C18 C19 1.382(6) . ? C19 C20 1.374(7) . ? C20 C21 1.395(7) . ? C21 C22 1.371(6) . ? O1W O2W 2.710(4) 3 ? O1W O3W 2.773(4) 4_565 ? O3W O5 2.916(6) 2_655 ? O2W O4 2.849(5) . ? N4 O6 1.182(6) . ? N4 O5 1.224(6) . ? N4 O4 1.240(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N2 88.08(12) . 1_455 ? O1 Co1 N1 88.17(12) . . ? N2 Co1 N1 176.15(14) 1_455 . ? O1 Co1 N3 163.98(14) . . ? N2 Co1 N3 87.73(13) 1_455 . ? N1 Co1 N3 95.65(13) . . ? O1 Co1 O1W 99.40(11) . . ? N2 Co1 O1W 95.92(13) 1_455 . ? N1 Co1 O1W 85.54(12) . . ? N3 Co1 O1W 96.42(13) . . ? O1 Co1 O2 57.79(11) . . ? N2 Co1 O2 89.85(12) 1_455 . ? N1 Co1 O2 87.42(12) . . ? N3 Co1 O2 106.73(13) . . ? O1W Co1 O2 156.36(10) . . ? C1 N1 C5 116.8(3) . . ? C1 N1 Co1 124.4(3) . . ? C5 N1 Co1 118.8(2) . . ? C6 N2 C10 117.2(3) . . ? C6 N2 Co1 122.3(3) . 1_655 ? C10 N2 Co1 120.5(3) . 1_655 ? C11 N3 C15 116.5(4) . . ? C11 N3 Co1 121.4(3) . . ? C15 N3 Co1 121.5(3) . . ? C16 O1 Co1 101.2(3) . . ? C16 O1 O2W 140.0(3) . . ? Co1 O1 O2W 118.25(14) . . ? C16 O2 Co1 80.5(3) . . ? C16 O2 O3W 158.4(3) . . ? Co1 O2 O3W 117.06(13) . . ? C20 O3 O5 109.0(3) . 4_556 ? N1 C1 C2 122.9(4) . . ? C1 C2 C3 120.2(4) . . ? C2 C3 C4 117.1(4) . . ? C2 C3 C8 120.7(4) . . ? C4 C3 C8 122.2(4) . . ? C5 C4 C3 119.4(4) . . ? N1 C5 C4 123.6(3) . . ? N2 C6 C7 122.6(3) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 117.3(4) . . ? C7 C8 C3 121.9(4) . . ? C9 C8 C3 120.8(4) . . ? C10 C9 C8 119.3(4) . . ? N2 C10 C9 123.6(4) . . ? N3 C11 C12 123.6(4) . . ? C11 C12 C13 120.3(4) . . ? C14 C13 C12 116.2(4) . . ? C14 C13 C13 122.1(5) . 3_565 ? C12 C13 C13 121.7(5) . 3_565 ? C13 C14 C15 120.6(4) . . ? N3 C15 C14 122.8(4) . . ? O2 C16 O1 120.2(4) . . ? O2 C16 C17 121.5(4) . . ? O1 C16 C17 118.3(4) . . ? C18 C17 C22 119.1(4) . . ? C18 C17 C16 119.4(4) . . ? C22 C17 C16 121.5(4) . . ? C19 C18 C17 120.2(5) . . ? C20 C19 C18 119.9(5) . . ? O3 C20 C19 117.2(5) . . ? O3 C20 C21 121.8(5) . . ? C19 C20 C21 121.0(5) . . ? C22 C21 C20 118.6(5) . . ? C21 C22 C17 121.3(4) . . ? Co1 O1W O2W 124.69(13) . 3 ? Co1 O1W O3W 112.28(14) . 4_565 ? O2W O1W O3W 102.10(14) 3 4_565 ? O2 O3W O5 80.97(15) . 2_655 ? O1 O2W O4 120.25(15) . . ? O6 N4 O5 120.9(6) . . ? O6 N4 O4 121.8(6) . . ? O5 N4 O4 117.3(5) . . ? N4 O4 O2W 116.8(4) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.555 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.069 #===END